A novel preparation route was developed for synthesizing SiO2/C nanocomposites through a mechanochemical-assisted sol-gel process combined with a high-energy dry ball milling process. The effect of process parameters, such as milling time, rotation speed and carbon content, on the structure and morphology of SiO2/C nanocomposites was investigated by X-ray diffraction, Fourier transform infrared spectroscopy, field-emission scanning electron microscopy and transmission electron microscopy with energy-dispersive spectroscopy. It was demonstrated from the physical characterization that the proposed preparation route might be an effective synthesis route for SiO2/C nanocomposites consisting of highly dispersed carbon nanoparticles on fine amorphous SiO2 particles. The electrochemical performance was characterized using Li vertical bar 1 M LiPF6 in EC: DMC = 1: 1 vertical bar SiO2/C cells in the potential range from 0.01 to 3.0 V versus Li/Li+. The SiO2/C nanocomposite prepared under optimized process conditions exhibited a highly stable reversible capacity of 663 mA h g(1) (872 mA h g-SiO21) at a current density of 46 mA g (1) after 30 cycles with no capacity fading. (C) 2014 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder